Progress 10/01/12 to 09/30/13
Outputs
Progress Report Objectives (from AD-416): ARS is interested in developing spectral fingerprinting methods for characterization and authentication of botanical dietary supplements. The Cooperator is interested in developing analytical methods for botanical materials. It has agreed to fund a 5-year proposal (FY2009-FY2013) submitted by FCMDL entitled �Development of spectral fingerprinting methods for rapid characterization and authentication of botanical dietary supplements�. Approach (from AD-416): FCMDL will develop methods for identification of Panax quinquefolium and Scutellaria lateriflora and characterization of authentic green tea, turmeric, cranberries, and opuntia (prickly cactus). Emphasis will continue to given to determining the efficacy of UV for identity methods. FCMDL will examine the many processed forms of P. ginseng. FCMDL will develop retention alignment programs that will allow application of pattern recognition to liquid chromatographic profiles in collaboration with the Ohio University (Athens,OH). In collaboration with the Office of Dietary Supplements at NIH, FCMDL is establishing an in-house database for phytochemical compounds, such as anthocyanins and other flavonoids, using high resolution mass spectrometry. To date, more than 300 compounds have been positively identified using the scientific literature and authentic reference materials. The new database contains their exact mass, chemical formula, structure, full mass spectra, and molecular absorption spectra. The database will be used to facilitate identification of chemical components in future analysis of food materials and will save significant time and resources. American ginseng (Panax quinquefolius) is far more expensive than Asian ginseng (P. ginseng) on the world market. Consequently, adulteration of American by Asian ginseng is common. FCMDL has developed an analytical method using a simple methanol-water extraction and direct analysis using flow injection mass spectrometry that can detect as little as 2% adulteration by Asian ginseng. In addition, a software model was developed that permitted adulterated spectra to be predicted based on the spectra of the pure American and Asian ginseng. Anthocyanins are common flavonoids that have been linked to resistance to cancer, diabetes, infections, inflammation, and neurological diseases. Scientists at USDA in Beltsville, MD, analyzed purple radishes (Raphanus sativus L.), a plant bred to provide high anthocyanin content, by high performance liquid chromatography ( HPLC) with high resolution mass detection (HRMS). The method detected 57 acylated anthocyanins, 45 for the first time. This study showed the presence of a large variety of anthocyanins and the necessity of HPLC-HRMS to provide the sensitivity and specificity for their identification. The popularity of botanical supplements to augment the US diet has provided a strong economic impetus for adulteration. Ginkgo biloba extract is a frequently used supplement that purportedly provides enhanced cognitive function. Scientists at USDA in Beltsville, MD, measured 22 flavonol glycosides in three NIST reference materials (SRM 3246, 3247, and 3248) and 20 commercially available supplements using HPLC-MS. Half of the commercial supplements were found to be adulterated with one of two inexpensive compounds (quercetin or quercetin rutinoside). Analysis was easily accomplished with a simple methanol-water extraction and direct analysis by UV spectrophotometry. This method provides the analyst with an inexpensive method for detecting adulterants. Samples of ten plants (sorghum, black beans, red beans, purple grape skin powder, soybeans, black cohosh, eggplant, corn flour, and broccoli) were extracted with three solvents (hexane, ethyl acetate, and methanol-water. All samples will be analyzed by HPLC-MS. This project will elucidate the extraction steps necessary for metabolomic profiling of plant materials.
Impacts
(N/A)
Publications
|
Progress 10/01/11 to 09/30/12
Outputs
Progress Report Objectives (from AD-416): ARS is interested in developing spectral fingerprinting methods for characterization and authentication of botanical dietary supplements. The Cooperator is interested in developing analytical methods for botanical materials. It has agreed to fund a 5-year proposal (FY2009- FY2013) submitted by FCMDL entitled �Development of spectral fingerprinting methods for rapid characterization and authentication of botanical dietary supplements�. Approach (from AD-416): FCMDL will develop methods for identification of Panax quinquefolium and Scutellaria lateriflora and characterization of authentic green tea, turmeric, cranberries, and opuntia (prickly cactus). Emphasis will continue to given to determining the efficacy of UV for identity methods. FCMDL will examine the many processed forms of P. ginseng. FCMDL will develop retention alignment programs that will allow application of pattern recognition to liquid chromatographic profiles in collaboration with the Ohio University (Athens,OH). In collaboration with Thermo Scientific and support from the Office of Dietary Supplements (ODS/NIH), FCMDL is establishing an in-house database for phytochemical compounds, such as anthocyanins and other flavonoids, using high resolution mass spectrometry. To date, more than 300 compounds have been positively identified using the scientific literature and authentic reference materials. The new database contains their exact mass, chemical formula, structure, full mass spectra, and molecular absorption spectra. The database will be used to facilitate identification of chemical components in future analysis of food materials and will save significant time and resources. Skullcap (Scutellaria lateriflora), is used as a dietary supplement and is an ingredient in numerous herbal products. It is routinely contaminated or adulterated with Germander (Teucrium canadense or Teucrium chamaedrys) due to the morphological similarities between the two genera. Unfortunately, Germander contains a compound that is hepatotoxic. A fast and reliable analytical method was developed using flow-injection mass spectrometry that can authenticate the purity of Skullcap in 1 minute. A brief survey of skullcap based dietary supplements revealed that 4 out of 13 were contaminated with germander. The project revealed that the commercially available skullcap based dietary supplements sold in the U.S. market are not safe and offers an easy and reliable method to identify unsafe products. American ginseng (Ginseng quinquefolius) is known worldwide as the purest, finest ginseng and is very important to the economy of Wisconsin. Unfortunately, American ginseng grown in China is being used to counterfeit Wisconsin ginseng. FCMDL has developed the first analytical method in the world, based on liquid chromatography, mass spectrometry, and pattern recognition mathematics that can differentiate between American ginseng grown in Wisconsin and China. This method can identify counterfeit American ginseng and can provide significant economical benefits to Wisconsin ginseng farmers. There are more than 8,000 flavonoid compounds in the plant kingdom. While current technology can identify these compounds it is impossible to obtain standards or maintain a standard inventory for quantifying all these compounds. FCMDL has developed an analytical scheme based on the common molecular absorption patterns of these compounds that allows quantification using a few inexpensive, commercially standards and easily determined molar relative response factors. The relative accuracy of the method is plus/minus 15%. High resolution mass spectrometry can readily identify all the flavonoids and this quantification scheme can determine their concentration.
Impacts
(N/A)
Publications
|
Progress 10/01/10 to 09/30/11
Outputs
Progress Report Objectives (from AD-416) ARS is interested in developing spectral fingerprinting methods for characterization and authentication of botanical dietary supplements. The Cooperator is interested in developing analytical methods for botanical materials. It has agreed to fund a 5-year proposal (FY2009- FY2013) submitted by FCMDL entitled �Development of spectral fingerprinting methods for rapid characterization and authentication of botanical dietary supplements�. This is the second year of the interagency grant. Approach (from AD-416) FCMDL will develop methods for identification of Panax quinquefolium and Scutellaria lateriflora and characterization of authentic green tea, turmeric, cranberries, and opuntia (prickly cactus). Emphasis will continue to given to determining the efficacy of UV for identity methods. FCMDL will examine the many processed forms of P. ginseng. FCMDL will develop retention alignment programs that will allow application of pattern recognition to liquid chromatographic profiles in collaboration with the Ohio University (Athens,OH). This is the third year of a 5-year interagency agreement with the Office of Dietary Supplements of the National Institutes of Health. In FY 2011, we continued using spectral fingerprinting and pattern recognition programs to compare the chemical composition of species of ginseng, black cohosh, ginkgo biloba, and scutellaria. We examined the pattern information available from infrared (IR), near-infrared (NIR), UV absorbance (UV), and mass spectrometry (MS). We determined that NIR and UV provide the most stable spectra, but MS offers the possibility of identifying specific compounds. The Office of Dietary Supplements (ODS) provided $150,000 in FY2010 towards the purchase of a high resolution mass spectrometry which provide core support for current and future analytical projects. We have begun a project to acquire representative spectra for specific botanicals and to characterize the natural variance of the spectra arising from growing year, growing site, and processing. We have demonstrated that fractions of the representative spectra can be mathematically summed and the level of adulteration predicted. We are in the process of experimentally verifying the model predictions. This agreement was monitored through routine conversations and e-mails with the Office of Dietary Supplements.
Impacts
(N/A)
Publications
|
Progress 10/01/09 to 09/30/10
Outputs
Progress Report Objectives (from AD-416) ARS is interested in developing spectral fingerprinting methods for characterization and authentication of botanical dietary supplements. The Cooperator is interested in developing analytical methods for botanical materials. It has agreed to fund a 5-year proposal (FY2009- FY2013) submitted by FCMDL entitled �Development of spectral fingerprinting methods for rapid characterization and authentication of botanical dietary supplements�. This is the second year of the interagency grant. Approach (from AD-416) FCMDL will develop methods for identification of Panax quinquefolium and Scutellaria lateriflora and characterization of authentic green tea, turmeric, cranberries, and opuntia (prickly cactus). Emphasis will continue to given to determining the efficacy of UV for identity methods. FCMDL will examine the many processed forms of P. ginseng. FCMDL will develop retention alignment programs that will allow application of pattern recognition to liquid chromatographic profiles in collaboration with the Ohio University (Athens,OH). This is the second year of a 5 year interagency agreement with the Office of Dietary Supplements of the National Institutes of Health. In 2010, we used spectral fingerprinting and pattern recognition programs to examine 3 species of ginseng roots (Panax ginseng aka �Chinese� ginseng, P. quinquefolius aka �American� ginseng, and P. notoginseng). More than 50 samples of the 3 species were obtained from the Ginseng Board of Wisconsin, American Herbal Pharmacopoeia, and several commercial sources (some authentic roots came directly from China). Mass spectrometry (MS) fingerprints acquired by direct analysis (root extracts with no chromatographic separation) readily identified the 3 species and the �red� and �white� preparations of the Chinese ginseng. Similar discrimination between species and preparations were obtained using UV absorption spectrophotometry and near infrared spectrometry. The latter method could discriminate between American ginseng grown in Wisconsin, Canada, and China. A follow-up study with 40 American ginseng roots from Wisconsin and China showed that MS could also discriminate between growing locations. Samples were analyzed by collaborating labs: Flora Research Lab (Grants Pass, OR) (1235-52000-060-06S) and the British Columbia Institute of Technology (Vancouver, Canada) (1235-52000-060-07S). This data will serve as the basis for a Single Laboratory Validated Method that will be submitted to AOAC International for certification as an official analytical method. This agreement was monitored through routine conversations and e-mails with the Office of Dietary Supplements.
Impacts
(N/A)
Publications
|
|